CN116023916A - Nanometer self-adaptive profile control and flooding agent and preparation method thereof - Google Patents
Nanometer self-adaptive profile control and flooding agent and preparation method thereof Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 claims abstract description 76
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 48
- 238000006243 chemical reaction Methods 0.000 claims abstract description 42
- 235000021122 unsaturated fatty acids Nutrition 0.000 claims abstract description 42
- 150000004670 unsaturated fatty acids Chemical class 0.000 claims abstract description 42
- 238000003756 stirring Methods 0.000 claims abstract description 39
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- 239000003960 organic solvent Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 18
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- 239000001257 hydrogen Substances 0.000 claims abstract description 17
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- 238000010438 heat treatment Methods 0.000 claims abstract description 16
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- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 14
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- 229910000271 hectorite Inorganic materials 0.000 claims abstract description 12
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- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 2
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- 235000020661 alpha-linolenic acid Nutrition 0.000 claims description 2
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Abstract
The invention discloses a nanometer self-adaptive profile control agent, which has the structural formula:wherein: n=2 to 8; m=6 to 20; r is a nanoparticle, and the nanoparticle is one of hydrotalcite-like nanoparticle, silicon dioxide nanoparticle, hectorite nanoparticle and oxidized metal nanoparticle. A method for preparing nanometer self-adaptive profile control agent comprises (1) mixing unsaturated fatty acid and alcohol, stirring at 20-60 deg. C for 4-8 h, cooling to room temperature to obtain reaction liquid; (2) Adding an organic solvent into the reaction solution, introducing hydrogen for at least 30min, heating to 30-80 ℃, and stirring and reacting for 1-4 h at the constant temperature to obtain the reaction solution; (3) Heating the reaction solution to 100-180 ℃, adding dimethylamine for mixing, stirring for 0.5-3 h, adding nano particles, continuously stirring for 2-5 h, and cooling to obtain the nano-particlesSelf-adaptive rice flooding agent.
Description
Technical Field
The invention relates to a profile control agent for oil field development, in particular to a nano self-adaptive profile control agent and a preparation method thereof.
Background
The profile control and flooding technology is taken as an important technical measure for improving the water flooding development effect and controlling water and stabilizing oil to realize stable production of the oil reservoir, can economically and effectively adjust and improve the heterogeneity of the oil reservoir, and has made an important contribution to the continuous stable production and high yield of the water flooding field.
However, when most oil reservoirs enter the middle and later stages of development, the influence of the heterogeneity of the oil reservoirs on the displacement effects of water flooding and chemical flooding is increasingly serious, the problem of heterogeneity is increasingly serious, large pore channels are increasingly developed, the residual oil is gradually dispersed, the profile control requirement of the high-temperature high-salt oil reservoir is increased, the conventional profile control effect is poor, and the oil reservoir has higher requirements on the profile control technology.
The self-emulsifying behavior of the self-adaptive profile control agent provides feasibility for deep profile control and plugging of dominant seepage channels. Droplets produced by self-emulsification can plug the formation by the gian effect and the highly elastic nature of the aggregates provides the opportunity for selective plugging. Meanwhile, the special performance of the self-adaptive material enables the displacement and plugging control of the displacement and flooding system, the positioning and placement of the displacement and flooding agent and the application to special oil reservoir environments to be possible.
The nanometer self-adaptive profile control agent has high reactivity and high coagulation energy, and the process is reversible, even if damaged, the reemulsification can be performed under certain conditions, and the reemulsification capability of the nanometer self-adaptive profile control agent provides possibility for long-term effective profile control system. The Chinese patent ZL 201410773016.6 provides a nano self-emulsifying system for profile control and flooding, which is water-in-oil nanoparticle sol, but the Chinese patent is water-in-oil emulsion, which has poor thermal stability and migration capability and cannot enter deep profile control and flooding of an oil layer.
Disclosure of Invention
The invention aims to: aiming at the defects of the prior art, the invention discloses a nano self-adaptive profile control and flooding agent and a preparation method thereof.
The technical scheme is as follows: a nanometer self-adaptive profile control agent has the structural formula:
wherein: n=2 to 8; m=6 to 20;
r is a nanoparticle, and the nanoparticle is one of hydrotalcite-like nanoparticle, silicon dioxide nanoparticle, hectorite nanoparticle and oxidized metal nanoparticle.
Further, the metal of the metal oxide nano-particles is one of titanium, zinc, aluminum, magnesium, iron, nickel and chromium, preferably titanium or zinc.
Still further, the nanoparticles are hectorite nanoparticles or hydrotalcite-like nanoparticles, preferably hectorite nanoparticles.
A preparation method of a nanometer self-adaptive profile control agent comprises the following steps:
(1) Mixing unsaturated fatty acid and alcohol, stirring at 20-60 ℃ for reaction for 4-8 hours, and cooling to room temperature to obtain a reaction solution;
(2) Adding an organic solvent into the reaction solution obtained in the step (1), introducing hydrogen for at least 30min, heating to 30-80 ℃, and stirring and reacting for 1-4 h at the constant temperature to obtain a reaction solution;
(3) Heating the reaction liquid obtained in the step (2) to 100-180 ℃, adding dimethylamine, mixing, stirring for 0.5-3 h, adding nano particles, continuously stirring for 2-5 h, and cooling to obtain the nano self-adaptive profile control agent.
Further, the unsaturated fatty acid in the step (1) is one or more of oleic acid, palmitoleic acid, ricinoleic acid, myristoleic acid, linoleic acid and linolenic acid.
Further, the alcohol in the step (1) is one or more of methanol, ethanol, propanol, ethylene glycol and glycerol.
Further, the weight ratio of unsaturated fatty acid to alcohol in the step (1) is 10 (1-8), and most preferably 10 (3-6).
Further, the organic solvent in the step (2) is one or more of m-xylene, toluene, benzene and xylene.
Further, the reaction temperature in the step (2) is 40-70 ℃ and the reaction time is 2-3 h.
Further, the organic solvent in the step (2) is 20% -50%, preferably 30% -45% of the weight of the unsaturated fatty acid.
Further, after the organic solvent is put into the reaction liquid obtained in the step (1) in the step (2), hydrogen is introduced for 0.5-2 h, then the temperature is raised to 40-80 ℃, and the introduction of hydrogen is stopped for 0.5-2 h after the reaction is finished.
And (3) heating the reaction liquid obtained in the step (2) to 120-170 ℃, adding dimethylamine, mixing, stirring for 1-2 h, adding nano particles, continuously stirring for 3-4 h, and cooling to obtain the nano self-adaptive profile control agent.
Further, dimethylamine in step (3) is 1 to 10% by weight, preferably 3 to 6% by weight, of unsaturated fatty acid.
Further, the nanoparticles in step (3) are 1 to 10% by weight, preferably 2 to 5% by weight, of the unsaturated fatty acid.
Further, the particle diameter of the nanoparticle in the step (3) is 10 to 50nm, preferably 20 to 45nm, more preferably 20 to 35nm.
Further, dimethylamine is added in the step (3) at least three times, and each time is separated by 20-40 min.
The hectorite nano-particles are disc-shaped particles with good monodispersity, the thickness of the particles is about 1nm, and the diameter is about 25nm. The magnesium oxide octahedral sheet is 2:1 layered silicate, two sides of the magnesium oxide octahedral sheet layer are respectively provided with a silicon oxide tetrahedral sheet which shares oxygen atoms with the magnesium oxide tetrahedral sheet, and part of Mg in a crystal lattice 2+ Is covered by Li + Displacing to make its surface have permanent negative charge with surface negative charge density of about 1.4e/nm 2 . Furthermore, when hectorite particles are dispersed in the aqueous phase, protonation of the hydroxyl groups at the edges of the particles can occur, resulting in small amounts of positive charge at the edges. The average chemical composition of laponite is: siO (SiO) 2 66.2%;MgO 30.2%;Na 2 O 2.9%;Li 2 O0.7%, the corresponding chemical formula is [ (Si) 8 (Mg 5.34 Li 0.66 )O 20 (OH) 4 ]Na 0.66 。
The dispersion of hectorite in water is good, and at lower concentrations, the aqueous dispersion of hectorite is in a transparent fluid state, and when the concentration of particles is greater than 2wt%, the dispersion rapidly forms a gel. The gel structure is formed mainly because the edges and the surfaces of clay particles are oppositely charged, and the surfaces of different particles are mutually attracted under the action of electrostatic attraction, so that the particles are mutually connected to form an edge-surface association structure, and the edge-surface association structure is further reinforced by Van der Waals effect, so that a card house type three-dimensional network structure is formed.
Hydrotalcite-like nanoparticles are represented by the general formula: [ M ] 2+ 1-x M 3+ x (OH) 2 ] x+ A n- x/n ·mH 2 O,
Wherein M is 2+ Refers to divalent metal cations, e.g. Mg 2+ ,Fe 2+ ,Ni 2+ ,Co 2+ ,Zn 2+ ;M 3+ Refers to trivalent metal cations, e.g. Al 3+ ,Cr 3+ ,Fe 3+ ,Co 3+ ,Ni 3+ The method comprises the steps of carrying out a first treatment on the surface of the x is the number of trivalent metal ions;a is an anion of valence n, e.g. Cl - ,OH - ,NO 3 - ,CO 3 2- ,SO 4 2- The method comprises the steps of carrying out a first treatment on the surface of the m is the number of interlayer water molecules. Preferably represented by the general formula: [ M ] 2+ 1-x M 3+ x (OH) 2 ] x+ A n- x/n ·mH 2 O, where M 2+ Refers to divalent metal cations Mg 2+ ;M 3+ Refers to trivalent metal cations Al 3+ The method comprises the steps of carrying out a first treatment on the surface of the x is the number of trivalent metal ions; a is an anionic Cl with a valence of n - ,OH - ,NO 3 - ,CO 3 2- ,SO 4 2- The method comprises the steps of carrying out a first treatment on the surface of the m is the number of interlayer water molecules; wherein the molar ratio of Mg to Al is 2:3.
The invention discloses a nanometer self-adaptive profile control agent and a preparation method thereof, which have the following beneficial effects:
1. the nano self-adaptive profile control agent is connected with nano particles in the synthesis process, so that the emulsifying property is enhanced, the nano particles can play a role in plugging at pore throats, the oil washing efficiency is improved, and the oil-water distribution can be regulated and controlled at a microcosmic level, so that the recovery ratio of a high-water-content oil reservoir is improved;
2. the preparation method is simple and is suitable for industrial production.
Drawings
FIG. 1 is a schematic diagram of a test apparatus for an indoor simulation test.
Fig. 2 is a schematic diagram of a synthetic route of the nano-adaptive profile control agent prepared in example 1.
Wherein:
1-advection pump | 2-pressure gauge |
3-intermediate container | 4-core barrel |
The specific embodiment is as follows:
the following detailed description of specific embodiments of the invention.
The reactions are all carried out in an atmospheric pressure reaction kettle, and chemicals are all commercially available.
In this application: the experiment of the indoor material model for improving the recovery ratio is carried out as follows:
1. test method
1) Measurement of permeability
In most formations the hydrocarbon water seepage is in accordance with Darcy's law, i.e
Q-seepage through sand layer, cm 3 /s
K-permeability of sand layer, darcy
A-seepage sectional area cm 2 Here the internal cross-section of the core barrel
DeltaL-distance cm between two seepage sections, here the length of the core tube
Mu-viscosity of liquid, centipoise
ΔP r The pressure difference is converted between the sections of the two seepage flows, and the converted pressure is equal to the actually measured pressure difference when the positions of the points are the same in height.
The permeability is then
Since the permeability is independent of the nature of the liquid, the permeability of the filled core barrel can be measured by water injection. When the viscosity of water is known, Δp is read by a pressure gauge, Q is calculated from the amount of discharged liquid and the discharge time, and a and Δl are both known values, the value of K can be obtained.
2. The test process comprises the following steps: saturated water, saturated oil and water are driven to contain 98 percent of water, the profile control agent 1PV is injected, and the subsequent water driving is finished to contain 98 percent of water.
3. Principle of testing
The test is carried out according to the actual condition of the oil field, the graph of the test device is shown in figure 1, and the saturated water permeability measurement is carried out on the glued core with certain permeability at first; then saturating the core with crude oil; in order to make the simulation test closer to the site, the core barrel is required to be subjected to crude oil aging, and the core barrel with saturated oil is placed in an oven at 80 ℃ for aging for about 48 hours; and (3) water flooding until the water content reaches 98%, then injecting a profile control agent flooding 1PV, injecting water for 0.1PV for displacement, and stopping the water flooding when the water content reaches 98%.
4. Test procedure
(1) The permeability K of the rock core is accurately measured by using clear water under the pump discharge capacity of 200mL/h and 300mL/h in sequence: three values are measured at each displacement, and the measurement is performed under the condition that the displacement is increased in sequence, because the larger the system displacement is, the larger the pressure difference between two ends of the core is, so that a large pore channel is easily formed in the core.
(2) Saturated crude oil: saturated oil was saturated at a pump displacement of 0.2mL/min until no water was present in the drained crude oil, and the amount of saturated oil was read by draining the volume of clean water.
(3) Aging of crude oil: the core tube was aged in an oven at 80℃for about 48 hours.
(4) The core tube is taken out and then placed in a constant-temperature water bath at 80 ℃, a pipeline is connected, and water flooding is carried out (note that the water flooding is uniformly set to have the discharge capacity of 0.2 mL/min): when the water is driven, a 10mL measuring cylinder is used for receiving the discharged liquid at the outlet end of the rock core, the pressure at full scale is recorded, the measuring cylinder is placed in a water bath, and the oil quantity and the water quantity are respectively read until the oil-water interface is clear. And (3) water is driven to the outlet of the core tube until the water content of the outlet liquid is about 98% (a 10mL measuring cylinder is used for receiving the outlet liquid at the outlet end of the core), and water injection is stopped.
(5) 0.2mL/min: after 1PV of flooding agent (with the concentration of 4000 mg/L) is filled into the clean and dry intermediate container, the intermediate container enters an oil displacement stage, the pump displacement is uniformly set to be 200mL/h, and the pressure, the oil quantity and the water quantity of the discharged liquid are recorded at intervals of about 10mL like water flooding.
(6) And (3) the following water flooding: the method is similar to the prior water flooding, and the water flooding is stopped when the number of the water flooding reaches 2-3 PVs.
(7) And calculating recovery ratio, wherein the oil quantity produced from the beginning of the injection system to the end of the subsequent water flooding is divided by the saturated oil quantity to improve the recovery ratio value.
Example 1
A preparation method of a nanometer self-adaptive profile control agent comprises the following steps:
(1) 1000kg of oleic acid is firstly added into a reaction kettle, 375kg of glycol is added under stirring, the temperature is raised to 40 ℃, the reaction kettle is stirred and reacts for 6 hours, and then the reaction kettle is cooled to room temperature to obtain reaction liquid;
(2) Pumping 250kg of m-xylene into the reaction liquid obtained in the step (1), stirring, introducing hydrogen for 30min, heating to 50 ℃, keeping the temperature unchanged, stirring and reacting for 2h to obtain the reaction liquid,
(3) Heating the temperature obtained in the step (2) to 160 ℃, adding 6.7kg of dimethylamine three times at intervals of 30min each time, stirring for 1h after the complete addition, adding 30kg of nano silicon dioxide particles, continuously stirring for 3h, and cooling to room temperature to obtain the nano self-adaptive profile control and flooding agent (namely the product).
The scheme for the synthesis of example 1 is shown in detail in FIG. 2.
The performance comparison of the nano-adaptive profile control agent prepared using the above examples with the currently commercially available emulsifiers commonly used in oil fields is shown in table 1 below.
The water for performance evaluation experiments is island oilfield produced water; the crude oil is produced from island oil field. The concentration used for evaluating the product properties was 0.4% by weight.
TABLE 1
From the above table, it can be seen that the nano self-adaptive profile control agent obtained in example 1 can self-emulsify crude oil, and the recovery ratio of the indoor material model after water flooding is greatly improved compared with that of the common emulsifying agent in oil field.
Example 2
A nanometer self-adaptive profile control agent has the structural formula:
wherein: n=2; m=6;
r is a nanoparticle, which is a hydrotalcite-like nanoparticle.
Example 3
A nanometer self-adaptive profile control agent has the structural formula:
wherein: n=8; m=20;
r is a nanoparticle, which is a silica nanoparticle.
Example 4
A nanometer self-adaptive profile control agent has the structural formula:
wherein: n=4; m=10;
r is a nanoparticle, which is a hectorite nanoparticle.
Examples 5 to 11
Substantially the same as in example 4, the only difference is that the nanoparticle R is different:
nanoparticles R | |
Example 5 | Titanium oxide nanoparticles |
Example 6 | Zinc oxide nanoparticles |
Example 7 | Alumina nanoparticles |
Example 8 | Magnesium oxide nanoparticles |
Example 9 | Iron oxide nanoparticles |
Example 10 | Nickel oxide nanoparticles |
Example 11 | Chromium oxide nanoparticles |
Example 12
A preparation method of a nanometer self-adaptive profile control agent comprises the following steps:
(1) Mixing unsaturated fatty acid and alcohol, stirring for 8 hours at 20 ℃, and cooling to room temperature to obtain a reaction solution;
(2) Adding an organic solvent into the reaction solution obtained in the step (1), introducing hydrogen for 30min, heating to 30 ℃, and stirring and reacting for 4 hours while keeping the temperature unchanged to obtain a reaction solution;
(3) And (3) heating the reaction liquid obtained in the step (2) to 100 ℃, adding dimethylamine for mixing, stirring for 0.5h, adding nano particles, continuously stirring for 2h, and cooling to obtain the nano self-adaptive profile control agent.
Further, the unsaturated fatty acid in step (1) is oleic acid.
Further, the alcohol in step (1) is methanol.
Further, the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:1, and in another embodiment, the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:3.
Further, the organic solvent in the step (2) is meta-xylene.
In another embodiment, the reaction temperature in step (2) is 40 ℃ and the reaction time is 3 hours.
Further, the organic solvent in the step (2) is 20% by weight of the unsaturated fatty acid. In another embodiment the organic solvent in step (2) is 30% by weight of unsaturated fatty acids.
In another embodiment, after the organic solvent is added into the reaction solution obtained in the step (1) in the step (2), 0.5 hydrogen is introduced first, and then the temperature is raised to 30 ℃, until 0.5h after the reaction is finished, the introduction of hydrogen is stopped.
In another embodiment, in the step (3), the reaction solution obtained in the step (2) is heated to 120 ℃, dimethylamine is added for mixing, nano particles are added after stirring for 2 hours, stirring is continued for 3 hours, and cooling is carried out, so that the nano self-adaptive profile control agent is obtained.
Further, dimethylamine in step (3) was 1% by weight of unsaturated fatty acid. In another embodiment, dimethylamine in step (3) is 3% by weight of unsaturated fatty acids.
Further, the nanoparticles in step (3) account for 1% by weight of the unsaturated fatty acid. In another embodiment, the nanoparticles in step (3) are 2% by weight of unsaturated fatty acids.
Further, the particle size of the nanoparticle in step (3) is 10nm. In another embodiment, the nanoparticle in step (3) has a particle size of 20nm.
Further, dimethylamine was added in three portions each of 20 minutes in step (3).
Further, the nanoparticle is a hydrotalcite-like nanoparticle
Example 13
A preparation method of a nanometer self-adaptive profile control agent comprises the following steps:
(1) Mixing unsaturated fatty acid and alcohol, stirring at 60 ℃ for reaction for 4 hours, and cooling to room temperature to obtain a reaction solution;
(2) Adding an organic solvent into the reaction solution obtained in the step (1), introducing hydrogen for at least 30min, heating to 80 ℃, and stirring to react 1 while keeping the temperature unchanged to obtain a reaction solution;
(3) And (3) heating the reaction liquid obtained in the step (2) to 180 ℃, adding dimethylamine for mixing, stirring for 0.5h, adding nano particles, continuously stirring for 5h, and cooling to obtain the nano self-adaptive profile control agent.
Further, the unsaturated fatty acid in the step (1) is palmitoleic acid.
Further, the alcohol in the step (1) is ethanol.
Further, the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:8. In another embodiment the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:6.
Further, the organic solvent in the step (2) is toluene.
Further, the reaction temperature in the step (2) was 70℃and the reaction time was 2 hours.
Further, the organic solvent in step (2) is 50% by weight of the unsaturated fatty acid, and in another embodiment the organic solvent in step (2) is 45% by weight of the unsaturated fatty acid.
In another embodiment, after the organic solvent is added into the reaction solution obtained in the step (1) in the step (2), hydrogen is introduced for 2 hours, and then the temperature is raised to 80 ℃, and the introduction of hydrogen is stopped for 2 hours after the reaction is finished.
And (3) heating the reaction liquid obtained in the step (2) to 170 ℃, adding dimethylamine, mixing, stirring for 2 hours, adding nano particles, continuously stirring for 4 hours, and cooling to obtain the nano self-adaptive profile control agent.
Further, dimethylamine in step (3) was 10% by weight of unsaturated fatty acid. In another embodiment the dimethylamine in step (3) is 3% by weight of unsaturated fatty acids.
Further, the nanoparticles in step (3) are 10% by weight of the unsaturated fatty acid. In another embodiment, the nanoparticles in step (3) are 2% by weight of unsaturated fatty acids.
Further, the particle size of the nanoparticle in step (3) is 50nm. In another embodiment, the nanoparticle in step (3) has a particle size of 45nm.
Further, dimethylamine was added in step (3) four times at 40min intervals.
Further, the nanoparticles in step (3) are silica nanoparticles.
Example 14
A preparation method of a nanometer self-adaptive profile control agent comprises the following steps:
(1) Mixing unsaturated fatty acid and alcohol, stirring at 40 ℃ for reaction for 6 hours, and cooling to room temperature to obtain a reaction solution;
(2) Adding an organic solvent into the reaction solution obtained in the step (1), introducing hydrogen for at least 30min, heating to 60 ℃, and stirring and reacting for 2h at the constant temperature to obtain a reaction solution;
(3) And (3) heating the reaction liquid obtained in the step (2) to 140 ℃, adding dimethylamine for mixing, stirring for 2 hours, adding nano particles, continuously stirring for 4 hours, and cooling to obtain the nano self-adaptive profile control and flooding agent.
Further, the unsaturated fatty acid in the step (1) is ricinoleic acid.
Further, the alcohol in the step (1) is glycerol.
Further, the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:5. In another embodiment, the weight ratio of unsaturated fatty acid to alcohol in step (1) is 10:4.
Further, the organic solvent in the step (2) is benzene.
In another embodiment, the reaction temperature in step (2) is 60 ℃ and the reaction time is 2.5h.
Further, the organic solvent in the step (2) is 35% by weight of the unsaturated fatty acid. In another embodiment, the organic solvent in step (2) is 40% by weight of unsaturated fatty acids.
In another embodiment, after the organic solvent is added into the reaction solution obtained in the step (1) in the step (2), hydrogen is introduced for 1h, and then the temperature is raised to 60 ℃ until the hydrogen is stopped to be introduced for 1h after the reaction is finished.
In another embodiment, in the step (3), the reaction solution obtained in the step (2) is heated to 150 ℃, dimethylamine is added for mixing, nano particles are added after stirring for 1.5 hours, stirring is continued for 3.5 hours, and then the nano self-adaptive profile control agent is obtained after cooling.
Further, dimethylamine in step (3) was 5% by weight of unsaturated fatty acid.
Further, the nanoparticles in step (3) are 4% by weight of the unsaturated fatty acid.
Further, the particle size of the nanoparticle in step (3) is 30nm.
Further, dimethylamine was added in five portions in step (3) at 25min intervals.
Further, step) (3) the nanoparticles are laponite nanoparticles.
Examples 15 to 20
Substantially the same as in example 12, except that the unsaturated fatty acid in step (1) was different:
examples 21 to 26
Substantially the same as in example 12, except that the alcohol in step (1) was different:
examples 27 to 31
Substantially the same as in example 12, except that the organic solvent in step (2) was different:
organic solvent in step (2) | |
Example 27 | Toluene (toluene) |
Example 28 | Benzene |
Example 29 | Xylene (P) |
Example 30 | Equal mass toluene and benzene mixed liquor |
Example 31 | Equal mass of mixed solution of meta-xylene, toluene, benzene and xylene |
Examples 32 to 38
Much as in example 14, the only difference is the nanoparticle:
the embodiments of the present invention have been described in detail. However, the present invention is not limited to the above-described embodiments, and various modifications may be made within the knowledge of those skilled in the art without departing from the spirit of the present invention.
Claims (15)
1. The nanometer self-adaptive profile control agent is characterized by comprising the following structural formula:
wherein: n=2 to 8; m=6 to 20;
r is a nanoparticle, and the nanoparticle is one of hydrotalcite-like nanoparticle, silicon dioxide nanoparticle, hectorite nanoparticle and oxidized metal nanoparticle.
2. A nano-adaptive profile control agent according to claim 1, wherein the metal of the metal oxide nano-particles is one of titanium, zinc, aluminum, magnesium, iron, nickel, chromium, preferably titanium or zinc.
3. A nano-adaptive profile control agent according to claim 1, wherein the nanoparticles are hectorite nanoparticles or hydrotalcite-like nanoparticles, preferably hectorite nanoparticles.
4. The preparation method of the nanometer self-adaptive profile control agent is characterized by comprising the following steps of:
(1) Mixing unsaturated fatty acid and alcohol, stirring at 20-60 ℃ for reaction for 4-8 hours, and cooling to room temperature to obtain a reaction solution;
(2) Adding an organic solvent into the reaction solution obtained in the step (1), introducing hydrogen for at least 30min, heating to 30-80 ℃, and stirring and reacting for 1-4 h at the constant temperature to obtain a reaction solution;
(3) Heating the reaction liquid obtained in the step (2) to 100-180 ℃, adding dimethylamine, mixing, stirring for 0.5-3 h, adding nano particles, continuously stirring for 2-5 h, and cooling to obtain the nano self-adaptive profile control agent.
5. The method for preparing a nano-adaptive profile control agent according to claim 4, wherein the unsaturated fatty acid in the step (1) is one or more of oleic acid, palmitoleic acid, ricinoleic acid, myristoleic acid, linoleic acid and linolenic acid.
6. The method for preparing a nano-adaptive profile control agent according to claim 4, wherein the alcohol in the step (1) is one or more of methanol, ethanol, propanol, ethylene glycol and glycerol.
7. The method of claim 4, wherein the weight ratio of unsaturated fatty acid to alcohol in the step (1) is 10 (1-8), and most preferably 10 (3-6).
8. The method for preparing a nano-adaptive profile control agent according to claim 4, wherein the organic solvent in the step (2) is one or more of meta-xylene, toluene, benzene and xylene.
9. The method of claim 4, wherein the reaction temperature in the step (2) is 40-70 ℃ and the reaction time is 2-3 h.
10. The method of claim 4, wherein the organic solvent in the step (2) is 20% -50%, preferably 30% -45% of the weight of the unsaturated fatty acid.
11. The method for preparing the nano self-adaptive profile control agent according to claim 4, wherein the reaction liquid obtained in the step (1) is put into an organic solvent in the step (2), hydrogen is introduced for 0.5-2 h, then the temperature is raised to 40-80 ℃ until the hydrogen is introduced for 0.5-2 h after the reaction is finished.
12. The method for preparing the nano self-adaptive profile control agent according to claim 4, wherein in the step (3), the reaction liquid obtained in the step (2) is heated to 120-170 ℃, dimethylamine is added for mixing, nano particles are added after stirring for 1-2 hours, and the nano self-adaptive profile control agent is obtained after cooling after continuing stirring for 3-4 hours.
13. The method of claim 4, wherein dimethylamine in step (3) is 1% -10%, preferably 3% -6% of the weight of unsaturated fatty acid.
14. The method of claim 4, wherein the nanoparticles in step (3) are 1-10% by weight, preferably 2-5% by weight, of the unsaturated fatty acid.
15. The method of claim 4, wherein the nanoparticle in step (3) has a particle size of 10-50 nm, preferably 20-45 nm, more preferably 20-35 nm;
and (3) adding dimethylamine at least three times, wherein each time is separated by 20-40 min.
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